反应详情

温度

70 °C

To a solution of 6-methoxy-2H-1,4-benzoxazin-3(4H)-one (Intermediate 48) (800 mg, 4.5 mmol) in DMF (16 mL) was added sodium hydride (60% in mineral oil, 260 mg, 6.5 mmol). After 20 minutes, (2-bromoethoxy)(tert-butyl)dimethylsilane (1.4 mL, 6.5 mmol) was added and it was heated to 70° C. in the microwave for 40 minutes. The reaction mixture was partitioned between water (100 mL) and ethyl acetate (100 mL). The aqueous phase was extracted with ethyl acetate (4×50 mL). The combined organic phases were washed with water (6×250 mL), dried over magnesium sulfate and concentrated at reduced pressure to afford the product as a yellow oil which was used without further purification. (1.38 g, 91%).

1. customThe reaction mixture was partitioned between water (100 mL) and ethyl acetate (100 mL)
2. extractionThe aqueous phase was extracted with ethyl acetate (4×50 mL)
3. washThe combined organic phases were washed with water (6×250 mL)
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated at reduced pressure